US10285405B2 - Oil carrying particulate matter and uses thereof - Google Patents

Oil carrying particulate matter and uses thereof Download PDF

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Publication number
US10285405B2
US10285405B2 US14/441,827 US201414441827A US10285405B2 US 10285405 B2 US10285405 B2 US 10285405B2 US 201414441827 A US201414441827 A US 201414441827A US 10285405 B2 US10285405 B2 US 10285405B2
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Prior art keywords
particulate matter
spp
oil
particles
beads
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US20150289520A1 (en
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Giora Kritzman
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NOBACTRA ISRAEL Ltd
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NOBACTRA ISRAEL Ltd
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    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N63/00Biocides, pest repellants or attractants, or plant growth regulators containing microorganisms, viruses, microbial fungi, animals or substances produced by, or obtained from, microorganisms, viruses, microbial fungi or animals, e.g. enzymes or fermentates
    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N25/00Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
    • A01N25/08Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests containing solids as carriers or diluents
    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N25/00Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
    • A01N25/12Powders or granules
    • A01N25/14Powders or granules wettable
    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N65/00Biocides, pest repellants or attractants, or plant growth regulators containing material from algae, lichens, bryophyta, multi-cellular fungi or plants, or extracts thereof
    • A01N65/08Magnoliopsida [dicotyledons]
    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N65/00Biocides, pest repellants or attractants, or plant growth regulators containing material from algae, lichens, bryophyta, multi-cellular fungi or plants, or extracts thereof
    • A01N65/08Magnoliopsida [dicotyledons]
    • A01N65/22Lamiaceae or Labiatae [Mint family], e.g. thyme, rosemary, skullcap, selfheal, lavender, perilla, pennyroyal, peppermint or spearmint
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B65CONVEYING; PACKING; STORING; HANDLING THIN OR FILAMENTARY MATERIAL
    • B65DCONTAINERS FOR STORAGE OR TRANSPORT OF ARTICLES OR MATERIALS, e.g. BAGS, BARRELS, BOTTLES, BOXES, CANS, CARTONS, CRATES, DRUMS, JARS, TANKS, HOPPERS, FORWARDING CONTAINERS; ACCESSORIES, CLOSURES, OR FITTINGS THEREFOR; PACKAGING ELEMENTS; PACKAGES
    • B65D75/00Packages comprising articles or materials partially or wholly enclosed in strips, sheets, blanks, tubes or webs of flexible sheet material, e.g. in folded wrappers
    • B65D75/28Articles or materials wholly enclosed in composite wrappers, i.e. wrappers formed by associating or interconnecting two or more sheets or blanks
    • B65D75/30Articles or materials enclosed between two opposed sheets or blanks having their margins united, e.g. by pressure-sensitive adhesive, crimping, heat-sealing, or welding
    • B65D75/32Articles or materials enclosed between two opposed sheets or blanks having their margins united, e.g. by pressure-sensitive adhesive, crimping, heat-sealing, or welding one or both sheets or blanks being recessed to accommodate contents
    • B65D75/36Articles or materials enclosed between two opposed sheets or blanks having their margins united, e.g. by pressure-sensitive adhesive, crimping, heat-sealing, or welding one or both sheets or blanks being recessed to accommodate contents one sheet or blank being recessed and the other formed of relatively stiff flat sheet material, e.g. blister packages, the recess or recesses being preformed
    • B65D75/367Articles or materials enclosed between two opposed sheets or blanks having their margins united, e.g. by pressure-sensitive adhesive, crimping, heat-sealing, or welding one or both sheets or blanks being recessed to accommodate contents one sheet or blank being recessed and the other formed of relatively stiff flat sheet material, e.g. blister packages, the recess or recesses being preformed and forming several compartments
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B65CONVEYING; PACKING; STORING; HANDLING THIN OR FILAMENTARY MATERIAL
    • B65DCONTAINERS FOR STORAGE OR TRANSPORT OF ARTICLES OR MATERIALS, e.g. BAGS, BARRELS, BOTTLES, BOXES, CANS, CARTONS, CRATES, DRUMS, JARS, TANKS, HOPPERS, FORWARDING CONTAINERS; ACCESSORIES, CLOSURES, OR FITTINGS THEREFOR; PACKAGING ELEMENTS; PACKAGES
    • B65D81/00Containers, packaging elements, or packages, for contents presenting particular transport or storage problems, or adapted to be used for non-packaging purposes after removal of contents
    • B65D81/32Containers, packaging elements, or packages, for contents presenting particular transport or storage problems, or adapted to be used for non-packaging purposes after removal of contents for packaging two or more different materials which must be maintained separate prior to use in admixture
    • B65D81/3261Flexible containers having several compartments
    • CCHEMISTRY; METALLURGY
    • C12BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
    • C12NMICROORGANISMS OR ENZYMES; COMPOSITIONS THEREOF; PROPAGATING, PRESERVING, OR MAINTAINING MICROORGANISMS; MUTATION OR GENETIC ENGINEERING; CULTURE MEDIA
    • C12N1/00Microorganisms, e.g. protozoa; Compositions thereof; Processes of propagating, maintaining or preserving microorganisms or compositions thereof; Processes of preparing or isolating a composition containing a microorganism; Culture media therefor
    • C12N1/20Bacteria; Culture media therefor
    • C12N1/205Bacterial isolates
    • C12R1/38
    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N25/00Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
    • A01N25/02Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests containing liquids as carriers, diluents or solvents
    • A01N25/04Dispersions, emulsions, suspoemulsions, suspension concentrates or gels
    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N25/00Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
    • A01N25/08Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests containing solids as carriers or diluents
    • A01N25/10Macromolecular compounds
    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N25/00Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
    • A01N25/34Shaped forms, e.g. sheets, not provided for in any other sub-group of this main group
    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N65/00Biocides, pest repellants or attractants, or plant growth regulators containing material from algae, lichens, bryophyta, multi-cellular fungi or plants, or extracts thereof
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B65CONVEYING; PACKING; STORING; HANDLING THIN OR FILAMENTARY MATERIAL
    • B65DCONTAINERS FOR STORAGE OR TRANSPORT OF ARTICLES OR MATERIALS, e.g. BAGS, BARRELS, BOTTLES, BOXES, CANS, CARTONS, CRATES, DRUMS, JARS, TANKS, HOPPERS, FORWARDING CONTAINERS; ACCESSORIES, CLOSURES, OR FITTINGS THEREFOR; PACKAGING ELEMENTS; PACKAGES
    • B65D81/00Containers, packaging elements, or packages, for contents presenting particular transport or storage problems, or adapted to be used for non-packaging purposes after removal of contents
    • B65D81/24Adaptations for preventing deterioration or decay of contents; Applications to the container or packaging material of food preservatives, fungicides, pesticides or animal repellants
    • CCHEMISTRY; METALLURGY
    • C12BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
    • C12RINDEXING SCHEME ASSOCIATED WITH SUBCLASSES C12C - C12Q, RELATING TO MICROORGANISMS
    • C12R2001/00Microorganisms ; Processes using microorganisms
    • C12R2001/01Bacteria or Actinomycetales ; using bacteria or Actinomycetales
    • C12R2001/38Pseudomonas

Definitions

  • the present disclosure concerns oil particulate products, for use, inter alia, in agriculture.
  • WO04034791 describes a controlled release composition
  • a controlled release composition comprising an essential oil having pesticidal and/or fungicidal properties, a supporting material therefor and means for controlling the release of the essential oil from the supporting material.
  • the composition is in the form of a free flowing powder.
  • the supporting material is one that may be a material, e.g. a powder material, that is capable of absorbing the essential oil to an extent that the resultant mixture is in the form of a free-flowing powder, such as clays and silicas, celites; zeolites.
  • the means for controlling the release of the essential oil from the supporting material is a high molecular weight, low melting wax or solid that is mixed with the support material.
  • particulate matter comprising particles carrying an essentially dry combination of components comprising at least one natural oil and at least one surfactant, the components being selected such that upon contact with water, an oil in water emulsion is formed.
  • the oil in water emulsion is a stable emulsion with no phase separation for at least 24 hours from its preparation.
  • the present disclosure also provides a composition comprising particulate matter as defined herein.
  • the composition comprises, in addition to the particulate matter, any adjuvant, additive, excipient etc., suitable and selected in accordance with the intended application.
  • the additional component may be one required to facilitate the use of the particulate matter in agriculture.
  • the particulate matter may comprise a single population of particles having one or more natural (e.g. essential) oils carried on the same particles, or a combination of populations, namely, one population of particles carried one type or one group of oils and at least one other population carrying another type or another group of oils, both types of population being as further discussed below.
  • natural oils e.g. essential oils
  • the at least one natural oil is one being characterized with anti-microbial activity.
  • the present disclosure also provides the use of the particulate matter as defined for the preparation of an anti-microbial emulsion.
  • the present disclosure provides a method of producing an anti-microbial emulsion comprising mixing the particulate matter with an aqueous solution to form said anti-bacterial emulsion.
  • the present disclosure provides a method of treating a plant, the method comprising, mixing the particulate matter with an aqueous solution to form an emulsion; and applying said emulsion onto at least part of the plant or to soil surrounding the plant.
  • the emulsion When requiring anti-microbial activity, the emulsion may be combined or used in combination with other anti-microbial agents as known in the art.
  • the present invention is based on the development of particulate material comprising a particulate carrier having absorbed thereon functional oils such that upon contact with water or water based solutions, a stable emulsion is formed.
  • the present disclosure provides particulate matter comprising particles carrying an essentially dry combination of components, the combination comprising at least one oil and at least one surfactant, and the components being selected such that upon contact with water, oil in water emulsion is formed.
  • the term “particulate matter” is used to denote a substance in the form of plurality of particle.
  • the particles may be in any particulate form, including, without limited thereto, from finely rounded beads to amorphous structures.
  • the particulate matter also includes any form of a powder.
  • the particulate matter comprise silica dioxide (SiO 2 , referred to herein as silica).
  • the silica may be naturally occurring silica particles such as bentonite clay beads, as well as synthetic silica beads, as known in the art.
  • the particulate matter comprises synthetic silica.
  • synthetic silica there is a variety of synthetic silica that may be used in the context of the present disclosure.
  • the particulate matter may comprise precipitated synthetic amorphous silica beads, such as the commercially available products Tixosil and Aerosil 200.
  • the particulate matter comprises synthetic or nature derived beads with a capacity to absorb natural oils.
  • Such beads may include, without being limited thereto Latex beads; calcium carbonate sorbent particle; cellulose beads; polystyrene adsorbents beads e.g. Amberlite® XAD®-2 which is a hydrophobic crosslinked polystyrene copolymer absorbent resin; charcoal; SepharoseTM beads; emulsan-alginate beads; chitosan beads; sodium alginate; styrene-maleic acid copolymer beads and styrene-divinylbenzene beads; cellulose paper beads.
  • Latex beads may include, without being limited thereto Latex beads; calcium carbonate sorbent particle; cellulose beads; polystyrene adsorbents beads e.g. Amberlite® XAD®-2 which is a hydrophobic crosslinked polystyrene copolymer absorbent resin; charcoal; SepharoseTM beads; e
  • the particulate matter has a size distribution in the range of 10-25 ⁇ m, at times 15 to 22 ⁇ m.
  • the particulate matter may also be characterized, without being limited thereto, by its surface area, in some embodiments, the particulate matter has a specific surface area (N 2 ) in the range of 400-550 m 2 /g, at times, in average 500 m 2 /g.
  • particulate matter may also be characterized, without being limited thereto, by its DBP absorption.
  • the DBP absorption (DOA absorption) is commonly used numerical value used to indicate absorption capacity of fillers and in the present disclosure indicates the oil capacity of the particulate matter.
  • the DBP is in the range of 250-350 ml/100 gram particles, at times, 280-320 ml/100 gram.
  • the first component comprises the particulate matter that holds one or a combination of natural oils.
  • natural oil encompasses any organic oil obtained from nature.
  • the natural oil is preferably oil derived from a plant.
  • the natural oils are essential oils.
  • Essential oils are preferably those known to exhibit antimicrobial (e.g. antibacterial) properties.
  • antimicrobial properties of the essential oils it is to be understood as being effective against any microbial pathogen, as further discussed below.
  • essential oils there are a variety of essential oils. Without being limited thereto, essential oils to be used in accordance with the present disclosure, may be those derived from the plants Origanum vulgare and Origanum spp., (e.g. Oregano), Mentha spp. (mint), Thymus spp. (Thyme), Myrtus spp., Ocimun spp. (e.g. Ocimun basilicum , also known as Basil), Lavandula spp. (e.g. Lavender), Micromeria spp., Coriandum spp. (e.g.
  • the natural oils are plant derived oils that are used as carbon source, e.g. as food/nutrient for the antagonistic microorganisms. These are referred to herein the term “carbon-base oil” or “carbon-rich nutrient oil”.
  • the carbon-base oils are vegetable oils. Without being limited thereto, the carbon-base oil is selected from the group consisting of Sesame oil, Olive oil, Peanut oil, Cottonseed oil, Soybean oil, Palm oil, sunflower oil, safflower oil, canola oil, castor oil, coconut oil, groundnut oil.
  • the natural oil is a combination of at least one essential oil and at least one carbon-base oil.
  • natural oil it is to be understood as also encompassing essential oil(s) and carbon-base oil(s).
  • the ratio between the at least one essential oil and at least one carbon-base oil is in the range of 60:40 and 100:0, at times the range is about 80:20.
  • each oil type is held separately on particulate matter such that different types of particulate matter are formed, each being characterized by the type of oil it is holding.
  • essential oil e.g. Oregano
  • carbon base oil e.g. Sesame
  • 80% carrying only essential oil such as Oregano
  • 20% carrying carbon base oil such as Sesame oil.
  • the particulate matter between 20% to 50% w/w of its total weight it provided by the oil loaded thereon.
  • the natural oil comprises at least Oregano oil in combination with at least one carbon-base oil.
  • the Oregano oil is combined, at times, with at least Sesame oil.
  • the amount of natural oils held by (absorbed by) the particles may vary, depending on the type(s) of natural oil used, the amount at loading, the type of particles used, the conditions of loading the natural oil onto the particulate matter, the surfactants and solvents used for loading etc.
  • the oil When referring to loading of oil onto the particles, it is to be understood as meaning any form of association between the oil and the particles (e.g. silica particles). Without being limited thereto, the oil is held by the particles by absorption onto and/or into the particles. The association between the particles and the oil is reversible, namely, under suitable conditions, such as when brought into contact with water, the oil is released from the particles to form an emulsion.
  • the present disclosure also provides a stable emulsion provided by said particulate matter, comprising the particles, at least one natural oil and at least one surfactant.
  • the particles hold between 20% to 50% w/w natural oil out of the total weight of the particulate matter (after loading). This is determined by conventional techniques such as HPLC or GC chromatography, as also exemplified below. In some other embodiments, the particles hold about 30% w/w natural oil at times, between 25-35%, at times between 28% to 32%, at times, around 30%.
  • the particulate matter also comprises at least one surfactant.
  • a surfactant is a compound that lowers the surface tension of a liquid and as such, the interfacial tension between two liquids to allow the formation of, e.g. an emulsion. It has been found by the inventors, as also shown in the following non-limiting examples, that the surfactant is essential in order to provide a stable emulsion, once the dry particulate matter is brought into contact with water.
  • the surfactant may be of any kind known in the art as safe for use (e.g. non-toxic to plants or animals) in agriculture.
  • the surfactant is a non-ionic surfactant, particularly those known to be suitable for agricultural applications.
  • a non-limiting list of possible non-ionic surfactants to be used in accordance with the present disclosure includes Polyethylene glycol sorbitan trioleates (Tween) such as Polyoxyethylenesorbitan Trioleate (Tween 85), Polyoxyethylenesorbitan Tristearate (Tween 65), sorbitan fatty acid esters, such as Sorbitan monopalmitate (Span 40)), Alcohol alkoxylate (BS1000).
  • Teween Polyethylene glycol sorbitan trioleates
  • Teween 85 Polyoxyethylenesorbitan Trioleate
  • Teween 65 Polyoxyethylenesorbitan Tristearate
  • sorbitan fatty acid esters such as Sorbitan monopalmitate (Span 40)
  • Alcohol alkoxylate BS1000
  • the surfactant comprises a salt of a fatty acid.
  • the salt may comprise an alkaline such as potassium, calcium, sodium salts, as well as an ammonium salt.
  • the salt of a fatty acid comprises potassium salts of fatty acids (also known as soap salts), which are typically uses as insecticides, herbicides, fungicides, and/or algaecides (these are at times considered non-ionic surfactants).
  • potassium salts of fatty acids may be obtained by adding potassium hydroxide to natural fatty acids such as those found in animal fats and in plant oils. Fatty acids may be extracted from vegetative sources such as olives, cotton seeds, soya beans, peanuts, sun flowers, coconuts Palm, Rapeseed, Sesame, Amaranth, Corn, Jatropha.
  • the fatty acid forming the surfactant may also be a synthetic fatty acid as well as a semi-synthetic (e.g. a natural fatty acid that underwent a modification).
  • the surfactant is one being recognized or is labeled as having an insecticide and/or fungicide activity.
  • pesticidal and/or fungicidal surfactants may include the commercial products Zohar PT-50 and Zohar LQ-215, both produced by Zohar Dalia, Israel.
  • the surfactant is selected from Zohar PT-50 and Zohar LQ-215.
  • compositions of these surfactants are available from Zohar Dalia.
  • Zohar PT-50 is known to have the following composition:
  • Vegetable oils Polyunsaturated fatty acids Mono- linolenic Linoleic Oleic Saturated unsaturated Total acid acid acid acid Smoke Type fatty acids fatty acids poly ( ⁇ -3) ( ⁇ -6) ( ⁇ -9) point Not hydrogenated Canola 7.365 63.276 28.14 9-11 19-21 — 204° C. (rapeseed) Coconut 91.00 6.000 3.00 — 2 6 177° C. Corn 12.948 27.576 54.67 1 58 28 232° C. Cottonseed 25.900 17.800 51.90 1 54 19 216° C. Flaxseed/ 6-9 10-22 68-89 56-71 12-18 10-22 107° C.
  • the amount of the surfactant may vary.
  • the particulate matter comprises between 5% to 10% w/w of one or a combination of surfactants.
  • the particulate matter is in an essentially dry form.
  • essential dry it is to be understood that the particulate matter is either completely dry (as determined by conventional methods) or contain low amounts of water, i.e. no more than 10% (w/w). In some other or additional embodiments, the water content in the particulate matter is within the range of 1% to 7% (w/w)).
  • the particulate matter may also contain some trace amounts of organic solvent(s).
  • the solvent is required for the preparation of the particulate matter and some residual amounts may remain in the final particulate matter.
  • the particulate matter comprises no more than 5%, 4%, 3% or even 2% w/w organic solvent.
  • the solvent is typically an organic volatile polar solvent, such as, without being limited thereto, a solvent selected from the group consisting of acetone, isopropyl alcohol, acetonitrile, ethanol and methanol.
  • the solvent is ethanol.
  • the particulate matter is unique in its capability of forming a stable emulsion, once the particulate matter is brought into contact with water.
  • a stable emulsion when referring to a stable emulsion it is to be understood as referring to dispersion of oil (the dispersed phase) in water (the dispersion medium) for a period of at least 1 hour, at times, at least 2, 3, 4, 5 or even 10 hours following the formation of the emulsion.
  • the stability is determined by the lack of visible separation into an oil phase and a water phase.
  • the particulate matter is mixed with water.
  • the amount of water depends on the amount of particulate matter.
  • water is added to provide a one liter emulsion.
  • 0.1 gr particulate matter provides an oil concentration of 0.03% v/v).
  • the percentage of oil in the final emulsion is in the range of 0.03% and 2% v/v.
  • the mixing of the particulate matter with water provides an emulsion with a droplet size in the range of between 1 to 20 ⁇ m and in some embodiments in the range between 3 to 10 ⁇ m.
  • the emulsion is an anti-microbial emulsion.
  • the particulate matter may be used as is or in combination with other ingredients, to form a composition comprising the particulate matter.
  • additional ingredients may depend on the intended use of the particulate matter.
  • the particulate matter may be combined with other dry powders including antimicrobial activity, additional dry surfactants.
  • the composition may comprise a single type (population) of particulate matter.
  • the particulate matter may comprise a combination of two or more populations of particulate matter, each population being different from the other at least in the type of essential oil absorbed therein.
  • the composition is a dry composition comprising dry particulate matter.
  • the present disclosure also provides a method of producing an anti-microbial emulsion comprising mixing the particulate matter or a composition comprising the particulate matter with an aqueous solution to form the emulsion, in particular, a stable emulsion.
  • the thus formed emulsion is characterized, inter alia, with formation of droplets, with an average droplet size in the range of 3 to 10 m.
  • the present disclosure also provides a method of treating a plant, the method comprises mixing particulate matter disclosed herein with an aqueous solution to form an emulsion and applying said emulsion onto at least part of the plant or to soil surrounding the plant.
  • the application of the emulsion may be by any means known in agriculture, including, without being limited thereto, spraying the plant, irrigation.
  • the treatment may include application onto the plant tubers, such as spraying of potato tubers (at times referred to as low spraying of tubers).
  • the emulsion may be applied to a plant in combination with other active principles, such as one or more antimicrobial agents.
  • the particulate matter is mixed with at least one antimicrobial agent prior to, concomitant with or subsequent to the formation of the emulsion.
  • the final emulsion (with or without additional active principles) may be applied to the plant once, twice or more times.
  • the doses may be provided with time intervals between applications of between one day interval to more than one days (two, three and more days interval).
  • the different doses may be the same or different.
  • Oregano oil with the following particulars: country of origin: Bulgaria; plant parts: flowering plant; cultivation method: certified organics, method of extraction: steam distilled.
  • Escherichia coli, Staphylococcus aureus, Salmonella, Clavibacter and Xanthomonas campestris were obtained from the collection of Prof. G. Kritzman Israel.
  • Bacteria were grown in nutrient broth test tubes at 27° C. for 24 hrs.
  • the paper discs were sterilized by autoclave in preparation for the disc diffusion method. Each bacteria (100 l), was placed on Nutrient agar (NA) plates and allowed to dry for 3-5 minutes.
  • the paper discs were saturated in 100% concentration of the oregano essential oil (20 ul), and then placed onto each NA plate freshly coated with bacteria.
  • the positive control used was 3% H 2 O 2 solution and the negative control was DI water.
  • the plates were incubated at 27° C. for 48 hours. The zone of inhibition was measured by standard ruler.
  • Oregano oil 100% essential oil
  • Sesame oil 100% carbon-base oil
  • Thymol, Carvacrol, Tween80, Tween 65, Tween R85 and Egg Lecithin all purchased from Sigma-Aldrich.
  • Span 40 purchased from Fluka, Israel.
  • Zohar LQ-215 (Potassium fatty acids) and Zohar PT-50 (Potassium fatty acids) purchased from Zohar Dalia.
  • Tixosil (SiO 2 ) purchased from Rhodia group.
  • Aerosil 200 and Sipernat 50S (SiO 2 , 20 ⁇ m) purchased from Evonik Industries AG.
  • Acetone and Acetonitrile purchased from J.T. Becker, Isopropanol (IPA), Gadot.
  • the powders containing the natural oils, surfactants and the silica beads were prepared using common lab glassware set up including laboratory bottles of 20-50 ml sizes, spatulas, magnetic stirrers and heating plates.
  • the natural oil was weight and each was separately mixed with the selected surfactant in a 20 ml vial, to which the solvent was added.
  • the mixtures of each oil were mixed and heated to a temperature of about 40 C until homogeneous solutions were obtained.
  • the silica beads were added until the liquid was absorbed by the beads.
  • the bottles were left in the fuming hood overnight until all solvent has evaporated.
  • Oregano oil based powder Surfactant Silica beads Solvent Form. No. Oregano oil Tween 80 Lecithin Tween 85 Tween 65 Span 40 Tixosil Aerosil 200 Acetone
  • ORG-18A 0.5 g 0.5 g 0.1 g 0.8 g 1 g
  • ORG-18B 0.5 g 0.5 g 0.1 g 0.8 g 1 g
  • ORG-18C 0.5 g 0.5 g 0.1 g 0.8 g 1 g
  • ORG-18D 0.5 gg 0.5 g 0.1 g 0.8 g 1 g ORG-20C 0.5 g 0.5 g 0.1 g 0.56 g 0.24 g 1 g ORG-20D 0.5 g 0.5 g g 0.1 g 0.4 g 0.4 g 1 g
  • Peristaltic pump 4.4 Carter 4/6 cassette manostat and tubing
  • the preparation included weighting and mixing the oil with the surfactant(s) in a 1 L beaker, to which isopropyl alcohol was added while mixing until a homogenous solution was obtained.
  • the silica beads (Sipernat 50S) were added to a 2 L beaker to which the homogenous solution was slowly (rate of 10 ml/min) added while mixing (30 rpm) until all liquid was absorbed into the beads.
  • Oregano oil based powder Surfactant Silica beads Solvent Form.
  • mixtures of powders (those containing Oregano oil and those containing Sesame oil) were prepared. Specifically, 400 g of formulation ORG-34 (beads carrying oregano oil) was mixed with 100 g of formulation SES-35 (beads carrying Sesame oil) in Dynamic Exim 5 L powder mixer at 10 rpm producing the mix O&S-A.
  • the mixed bead powders were used as is.
  • IPA content was determined using a headspace analysis according to the parameters bellow:
  • Impurities profile were determined in accordance with the method reported by H. Hajimehdipoor “A validated high performance liquid chromatography method for the analysis of thymol and carvacrol in Thymus vulgaris L. volatile oil” in Pharmacogn Mag. 2010 July-September; 6(23): 154 158 and adopted by SoluBest.
  • Nucleosil 100 C18 HD, 3 ⁇ , 150 ⁇ 3 mm column and Ultimate 3000 Dionex (Germany) HPLC system with photodiode array (PDA) detectors and Chromeleon Version 6.80 software packages were used.
  • the mobile phase is Acetonitrile:Water (50:50, v/v). Minimum resolution between Carvacrol and Thymol peaks is 1.5.
  • Thymol and 20 mg Carvacrol were weighted into 50 mL volumetric flask, and dissolved in 40 mL of diluents, then brought up to volume with the diluent and mixed.
  • the resulting concentration of the Thymol standard solution was about 0.06 mg/mL and Carvacrol standard solution was about 0.4 mg/mL.
  • Sesame oil absorbed on silica beads was trans-methylated overnight with methanolic HCl solution at 60° C.
  • Heptadecanoic acid used as an internal standard, was added to beads before derivatization.
  • Methyl esters of fatty acids were extracted with hexane and dried over anhydrous sodium sulfate prior to GC analysis.
  • Calibration standards were prepared from different concentrations of sesame oil and blank beads. Conditions of derivatization and amount of internal standard were the same as described in sample preparation.
  • Table 5 provides the % of Sesame oil in the formulation as determined by GC Chromatograph.
  • the water content measured using Karl Fisher titration found that the powder contains 5-7% of water. It appears the source of the water is from Zohar PT 50 surfactant, which contents 50% of water.
  • the amount of IPA varies from 5 to 13%. However, in the field, the formulations were diluted for at least 30 times and as such, the content of IPA was reduced to 0.17-0.43%, which is negligible and very safe amount.
  • the different types of dry powders prepared showed stable after long term (more than a year) storage. In addition to the above, it is noted that the powders have a characteristic odor.
  • the oregano oil based formulations have off-white color and sesame oil based powders are white.
  • Assay of sesame oil was measured via two major constituents—C16:0 and C18:0—in the beginning of the stability study (initial point) and after 8 weeks using GC-FID analysis of methylated fatty acids. Trans methylation was performed upon acidic catalysis (with MeOH/HCl) using C17:0 as an internal standard. The obtained values were normalized to the amounts of markers in the pure sesame oil.
  • Isopropanol content was tested using GC method.
  • the amount of IPA was reduced on 36% after 8 weeks of storing in accelerating conditions in oregano formulation, but it was preserved in the sesame formulation.
  • the containers were leaky and in order to reduce water or IPA loss, the containers may be more hermetically sealed.
  • a surfactant emulsifying agent
  • HLB HLB 8-20
  • two surfactants were tested Tween 80 having an HLB value of 15 and potassium salt of fatty acids extracted from palm, coconut, olive, castor and cottonseed plants (potassium salt oleate having an HLB value of 20).
  • the tested emulsifiers included: Tween 20; Tween 80; Triton X 100; Lecithin; SDS; Sodium Stearate and Potassium fatty acid. Each emulsifiers was tested at the following concentrations (in percentage) 1; 5; 10; 15; 20 for a mixture of water containing 25% oregano oil with 5% sesame oil.
  • the stability during the first 24 hours (i.e. lack of phase separation) and anti-bacterial activity of each emulsion were determined.
  • Anti bacterial activity was determined by measuring the inhibition zones of 20 l emulsion towards the following plant pathogenic bacteria: Clavi bacter; Xanthomonas and Streptomyces spp. and by spraying the emulsions on pepper plants as test plants for phytotoxicity symptoms.
  • the oregano oil and surfactant were absorbed on silica beads (with the air of isopropanol, as described above). Good anti-bacterial results were obtained when 0.5% of oregano-based powder was dispersed in water. This powder contained about 25% of oregano oil and 10% of potassium fatty acids emulsifier, namely, a concentration of 0.125% oregano oil in emulsion was active enough and needed only 0.05% of surfactant to be solubilized from the powder form.
  • SiO 2 particles Sipernet 50S (20 m, Evonik Industries, lot 1462)
  • the oregano oil and sesame oil were mixed, to which IPA was added until a homogenous solution was obtained.
  • the surfactant was added by mixing until a non-viscous homogenous solution was obtained.
  • the solution was sprayed on the SiO 2 powder and mixing was peformed using low sheer force equipment until all liquid was absorbed and continued for an additional period of 15-30 min. Then the powder was grind to breakdown aggregates and sieved through mesh 1,000 m.
  • the bag containing the powder was hermetically sealed and stored. Storage was for at least 2 years, at 15-30 C.

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CA2907945A1 (en) 2014-10-23
BR112015026387A2 (pt) 2017-07-25
EP2986110A1 (en) 2016-02-24
US20190254286A1 (en) 2019-08-22
MA38525B2 (fr) 2019-05-31
MX2015014638A (es) 2016-05-31
RU2614063C1 (ru) 2017-03-22
JP2016522174A (ja) 2016-07-28
US20150282491A1 (en) 2015-10-08
JP2016515646A (ja) 2016-05-30
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US20150289520A1 (en) 2015-10-15
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